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采用间苯二酚为原料,经过磺化、硝化、水解合成2-硝基-1,3-苯二酚,再用硫酸二甲酯进行甲基化,得到2-硝基-1,3-苯二甲醚。重点讨论了2-硝基1,3-苯二酚及其甲醚化工艺条件,结果表明,使用质量分数20%发烟硫酸可使1,3-苯二酚全部二磺化从而使2-硝基1,3-苯二酚收率增至63.5%,色谱纯度达98.5%以上;在反应温度80℃,反应时间4 h,n(M e2SO4)∶n(2-硝基1,3-苯二酚)=2.2∶1.0时,2-硝基-1,3-苯二酚甲基化收率高达75.6%。
Using resorcinol as raw material, sulfonation, nitration, hydrolysis of 2-nitro-1,3-benzenediol, and then methylated with dimethyl sulfate to give 2-nitro- Xylene dimethyl ether. The conditions of 2-nitro-1, 3-benzenediol and its methyl etherification were discussed. The results showed that the use of 20% oleum could disulfonate 1,3-benzenediol and make 2- The yield of nitro-1,3-benzenediol increased to 63.5% and the chromatographic purity reached 98.5%. Under the conditions of reaction temperature 80 ℃, reaction time 4 h, n (M 2 SO 4) Benzenediol) = 2.2:1.0, the yield of 2-nitro-1,3-benzenediol was as high as 75.6%.